US10644350B2 - Secondary battery including organic-inorganic hybrid nanoporous material as water adsorbent - Google Patents
Secondary battery including organic-inorganic hybrid nanoporous material as water adsorbent Download PDFInfo
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- US10644350B2 US10644350B2 US15/924,033 US201815924033A US10644350B2 US 10644350 B2 US10644350 B2 US 10644350B2 US 201815924033 A US201815924033 A US 201815924033A US 10644350 B2 US10644350 B2 US 10644350B2
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- organic
- inorganic hybrid
- water
- hybrid nanoporous
- nanoporous material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Definitions
- the present invention relates to a secondary battery comprising an organic-inorganic hybrid nanoporous material as a water adsorbent.
- lithium secondary batteries having high energy density and voltage, a long cycle life, and a low self-discharge rate have been commercialized and widely used.
- the lithium secondary batteries are largely classified into a cylinder-type battery, a polygon-type battery, and a pouch-type battery according to their shape, and also classified into a lithium ion battery, a lithium ion polymer battery, and a lithium polymer battery according to the type of an electrolyte.
- water may be included inside an active material or a small amount of water may exist in an electrolyte, and particularly, in the case of the pouch-type case, water is very likely to penetrate through sealing parts, etc.
- water and the electrolyte react with each other by a potential energy provided during a charging process, which causes the battery to swell due to gas generation.
- water in the battery reacts with components of the battery to generate reaction products, such as HF, etc.
- HF destroys SEI layer and causes dissolution of a cathode. This phenomenon occurs more remarkably at a high temperature so that serious problems may be generated in terms of safety of the battery.
- LiPF 6 lithium salts which are mainly used in high-voltage and high-capacity batteries, react with water to form a strong acid HF.
- the formed HF spontaneously reacts with a weakly basic electrode active material to elute the electrode active material components, resulting in degradation of the battery.
- HF forms lithium fluoride (LiF) on the surface of the cathode to increase electric resistance in the electrode and to generate gas, leading to a reduction of the lifetime of the battery.
- HF reacts with a silicon (Si) component of a glass container, which is commonly used for electrolyte preparation, to produce silicon precipitates.
- the silicon precipitates thus produced are adsorbed onto the surface of the battery during charge/discharge of the battery, thereby reducing a reaction area.
- charge/discharge efficiency of the battery is rapidly reduced, and consequently, the life-time of the battery is reduced due to reaction with the electrode.
- a predetermined concentration usually, 150 ppm
- HF may cause a rapid oxidation reaction, thereby deteriorating performance of the anode.
- an active material slurry is coated onto an electrode and then dried by hot air, etc., thereby removing a solvent and water in the slurry coated onto a metal current collector.
- water removal in the electrode active material composition is more problematic because of high water absorption and difficulty of water removal due to the nature of the material.
- a water adsorbent is introduced inside a secondary battery to prevent side reactions by water, thereby improving reliability of the battery.
- FIG. 1 shows a structure of Al(OH)BDC organic-inorganic hybrid nanoporous material
- FIG. 2 shows result of X-ray diffraction analysis of Al(OH)BDC organic-inorganic hybrid nanoporous material
- FIG. 3 shows a thermogravimetric analysis graph of Al(OH)BDC sample, which was measured from room temperature to 700° C. at a heating rate of 5° C. per minute under nitrogen atmosphere;
- FIG. 4 shows a nitrogen physical adsorption isotherm for Al(OH)BDC organic-inorganic hybrid nanoporous material, which was measured at a liquid nitrogen temperature ( ⁇ 195° C.);
- FIG. 5 shows a water adsorption/desorption isotherm for Al(OH)BDC, which was measured at 30° C.
- FIG. 6 shows result of X-ray diffraction analysis of Al-Fumarate organic-inorganic hybrid nanoporous material
- FIG. 7 shows a thermogravimetric analysis graph of Al-Fumarate sample, which was measured from room temperature to 700° C. at a heating rate of 5° C. per minute under nitrogen atmosphere;
- FIG. 8 shows a nitrogen physical adsorption isotherm for Al-Fumarate organic-inorganic hybrid nanoporous material, which was measured at a liquid nitrogen temperature ( ⁇ 195° C.);
- FIG. 9 shows result of X-ray diffraction analysis of MIL-100(Fe) organic-inorganic hybrid nanoporous material
- FIG. 10 shows a thermogravimetric analysis graph of Al-Fumarate sample, which was measured from room temperature to 650° C. at a heating rate of 5° C. per minute under nitrogen atmosphere;
- FIG. 11 shows a nitrogen physical adsorption isotherm for MIL-100(Fe) organic-inorganic hybrid nanoporous material, which was measured at a liquid nitrogen temperature ( ⁇ 195° C.);
- FIG. 12 shows a water adsorption/desorption isotherm for MIL-100(Fe), which was measured at 30° C.
- FIG. 13 shows result of a water adsorption test of LiFePO 4 cathode active material including 10% by weight of Al(OH)BDC under air flow at a relative humidity of 10%;
- FIG. 14 shows result of a water adsorption test of LiFePO 4 cathode active material including 10% by weight of Al-Fu under air flow at a relative humidity of 10%;
- FIG. 15 shows result of a water adsorption test of LiFePO 4 cathode active material including 10% by weight of MIL-100(Fe) under air flow at a relative humidity of 10%.
- FIG. 16 shows a schematic diagram of a secondary battery having metal-organic framework as an adsorbent according to an embodiment of the present invention.
- a first aspect of the present invention provides a secondary battery having a battery case which accommodates an electrode assembly including a cathode, an anode, and a separator disposed between the cathode and the anode, together with an electrolyte, wherein one or more selected from the group consisting of the cathode, the anode, the separator, the electrolyte, and the interior of the battery case include a first organic-inorganic hybrid nanoporous material as a water adsorbent which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower.
- the secondary battery may be a lithium ion battery, a lithium ion polymer battery, or a lithium polymer battery.
- a second aspect of the present invention provides a battery module including the secondary battery according to the first aspect as a unit battery.
- a third aspect of the present invention provides a battery pack including the battery module according to the second aspect.
- a fourth aspect of the present invention provides a device including the battery pack according to the third aspect as a power source.
- a fifth aspect of the present invention provides an electrolyte including, as a water adsorbent, a first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower; a second organic-inorganic hybrid nanoporous material, of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less (herein, p0 represents a saturated vapor pressure at an application temperature and p represents a vapor pressure upon adsorption); or both of them.
- a sixth aspect of the present invention provides an electrode active material composition including, as a water adsorbent, a first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower; a second organic-inorganic hybrid nanoporous material, of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less (herein, p0 represents a saturated vapor pressure at an application temperature and p represents a vapor pressure upon adsorption); or both of them.
- a seventh aspect of the present invention provides a method of manufacturing a water-removed secondary battery having a battery case which accommodates an electrode assembly including a cathode, an anode, and a separator disposed between the cathode and the anode, together with an electrolyte, the method including the step of adsorbing water during manufacturing of the battery and desorbing water during assembling of the battery by using a first organic-inorganic hybrid nanoporous material as a water adsorbent which may be regenerated by desorbing 70%, or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower.
- inorganic porous materials such as zeolite, mesoporous, clay, etc have been mainly reported as water adsorption materials.
- Water adsorption properties of the porous materials may be divided into 4 kinds, based on change of adsorption amount according to relative humidity in a water (H 2 O) isotherm.
- a water H 2 O
- an adsorbent strongly adsorbing water shows a rapid increase in the water adsorption amount at a relative humidity (p/p0) of 0.1 or less (a representative porous material is zeolite having micropores).
- An adsorbent having a moderate water adsorption strength shows a rapid increase in the water adsorption amount at a relative humidity (p/p0) of 0.1 to 0.3.
- An adsorbent having a water adsorption strength slightly lower than the moderate water adsorption strength shows a rapid increase in the water adsorption amount at a relative humidity (p/p0) of 0.3 to 0.6.
- An adsorbent having a weak water adsorption strength such as activated carbon shows a rapid increase in the water adsorption amount at a relative humidity (p/p0) of 0.7 or more.
- water desorption properties tend to be opposite to the water adsorption properties.
- water desorption may occur at a high temperature of 200° C. or higher, and in the case of materials having a moderate to slightly low water adsorption strength such as organic-inorganic hybrid nanoporous materials, water desorption may occur at 150° C. or lower.
- the degree of desorption may differ depending on the adsorption properties according to the kind of the organic-inorganic hybrid nanoporous material.
- the device in order to use the water adsorbent for an electronic device, the device must be assembled after readily removing water during a process of introducing the water adsorbent into the electronic device, because most manufacturing processes include a certain amount of water.
- the adsorption and desorption properties are opposite to each other, for example, zeolite has an advantage of high adsorption strength, whereas desorption does not easily occur during the process of manufacturing the device, and desorption easily occurs at a high temperature. Therefore, when the high-temperature heat treatment is difficult due to the characteristics of the device, zeolite cannot be used.
- the first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower is used as a water adsorbent in a secondary battery
- the material acts as the water adsorbent to adsorb water during manufacturing of the secondary battery, and then easily desorbs water by vacuum-treatment at a relatively low temperature of 150° C. or lower during assembling of the battery, thereby removing water from the battery.
- the organic-inorganic hybrid nanoporous material has a relatively low water adsorption strength at a low humidity, but it may show desorption at a low temperature, and therefore, the electronic device may be manufactured in a state where water is readily removed in the process of manufacturing the device.
- the first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower may belong to adsorbents having a moderate or slight low water adsorption strength, which show a rapid increase in the water adsorption amount at a relative humidity (p/p0) ranging from 0.2 to 0.6, as described above.
- the water adsorbent inside the assembled electronic device is required to have a property of not readily desorbing the adsorbed water during operation of the electronic device.
- the adsorbent having a moderate or slight low water adsorption strength i.e., the first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower may desorb gas components (moisture or carbon dioxide) adsorbed during operation of the electronic device even at a low temperature.
- the first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower may desorb gas components (moisture or carbon dioxide) adsorbed during operation of the electronic device even at a low temperature.
- the amount of water adsorbed from air during the process of manufacturing the device is large and the amount of water included in the electronic device during operation of the electronic device is very small (approximately ⁇ 5%), and therefore, it is difficult to satisfy all the requirements by using only one kind of the organic-inorganic hybrid nanoporous material.
- a second organic-inorganic hybrid nanoporous material of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less (herein, p0 represents a saturated vapor pressure at an application temperature and p represents a vapor pressure upon adsorption), is further used, in addition to the first organic-inorganic hybrid nanoporous material, and as a result, the second organic-inorganic hybrid nanoporous material may effectively adsorb but may not desorb several hundreds of ppm of water which may be generated during operation of the battery, or desorbed gas components derived from the first organic-inorganic hybrid nanoporous material. Accordingly, side reactions caused by desorbed gas may be suppressed even during operation of the electronic device, thereby providing an electronic device having higher stability and reliability.
- the first organic-inorganic hybrid nanoporous material and the second organic-inorganic hybrid nanoporous material are used in combination in the secondary battery, and thus they act as the water adsorbent to adsorb water during manufacturing of the secondary battery, and then readily desorb water by vacuum-treatment at a relatively low temperature of 150° C. or lower during assembling of the battery, thereby easily removing water from the battery. Subsequently, it is possible to effectively adsorb water generated inside the battery even at a low relative humidity of the battery during operation of the battery, thereby improving reliability of the battery.
- organic-inorganic hybrid nanoporous materials are also called “porous coordination polymers” [Angew. Chem. Intl. Ed., 43, 2334, 2004], or “metal-organic frameworks (MOF)”.
- the organic-inorganic hybrid nanoporous material may be defined as a porous organic-inorganic polymer compound formed by binding a central metal ion to an organic ligand via a molecular coordination bond, and the organic-inorganic hybrid nanoporous material refers to a crystalline compound with molecular-sized or nano-sized pores, including both organic material and inorganic material in its framework structure.
- a polar metal ion and a carboxylate oxygen anion are both included in its crystalline framework, and a non-polar aromatic compound group coexists therein, and therefore, hydrophilicity and hydrophobicity are exhibited at the same time.
- the organic-inorganic hybrid nanoporous materials have a large surface area and molecular-sized or nano-sized pores, and thus may be used for encapsulating guest molecules smaller than their pore size or separating molecules according to the sizes of the molecules by using their pores.
- the secondary battery according to the present invention is a secondary battery having a battery case which accommodates an electrode assembly including a cathode, an anode, and a separator disposed between the cathode and the anode, together with an electrolyte, wherein one or more selected from the group consisting of the cathode, the anode, the separator, the electrolyte, and the interior of the battery case may include the first organic-inorganic hybrid nanoporous material as a water adsorbent which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower.
- the first organic-inorganic hybrid nanoporous material as a water adsorbent which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower.
- first organic-inorganic hybrid nanoporous material may refer to, as described above, an organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70° % or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower
- the first organic-inorganic hybrid nanoporous material may be regenerated by desorbing 50% or more of the total adsorption amount of adsorbed water at 100° C. or lower.
- the first organic-inorganic hybrid nanoporous material may adsorb 50% or more of the total adsorption amount of water at a relative humidity p/p0 ranging from 0.3 to 0.6.
- the first organic-inorganic hybrid nanoporous material may be an organic-inorganic hybrid nanoporous material having 0.5 mol to 3 mol of a hydrophilic hydroxyl group (OH) or a hydroxide anion (OH ⁇ ) group as a ligand per 1 mol of a central metal ion in a nanopore.
- the first organic-inorganic hybrid nanoporous material has a water adsorption capacity of 0.15 gram or more per 1 gram or 1 milliliter thereof.
- representative examples of the first organic-inorganic hybrid nanoporous material may include aluminum fumarate, zirconium fumarate, CAU-10, MIL-160, MIL-53, UiO-66, analogs thereof, etc.
- the first organic-inorganic hybrid nanoporous material having a hydrophilic OH ligand which is weaker than the coordinatively unsaturated metal site in the framework, exhibits a not very strong interaction with polar molecules such as water
- the first organic-inorganic hybrid nanoporous material may be not only effective as a water adsorbent, but also regenerated by desorbing water at a low temperature.
- the content of the hydrophilic hydroxyl group (OH) or the hydroxide anion (OH ⁇ ) group is less than 0.5 mol per 1 mol of the central metal ion, hydrophilicity may be weak, and therefore, the water adsorption amount at a low relative humidity may be not high, and when the content is more than 3 mol per 1 mol of the central metal ion, hydrophilicity may be too strong, and therefore, water desorption may not easily occur to increase a regeneration temperature.
- the first organic-inorganic hybrid nanoporous material is preferably a material which does not react with the electrolyte and the electrode active material and does not deteriorate performances of the battery particularly, in the first organic-inorganic hybrid nanoporous material, the central metal ion is preferably a central metal ion that does not electrochemically react in the secondary battery.
- the central metal ion is preferably a central metal ion that is free of sites for reaction/adsorption with lithium ions because of having no unshared electron pairs.
- the first organic-inorganic hybrid nanoporous material according to the present invention preferably has a center metal ion which does not significantly lower the lithium ion mobility, thereby suppressing the decrease of conductivity and the deterioration of battery performance. Therefore, in the first organic-inorganic hybrid nanoporous material according to the present invention, the central metal ion is preferably not a transition metal, because the transition metal may react with or encapsulate lithium ions.
- the ligand is not critical and the central metal ion is preferably one or more selected from the group consisting of aluminum ion, calcium ion, gallium ion, indium ion, magnesium ion, and zirconium ion.
- the size of the nanopore of the first organic-inorganic hybrid nanoporous material may be controlled by adjusting the length and/or type of the ligand.
- the first organic-inorganic hybrid nanoporous material according to the present invention may have heterocyclic dicarboxylic acid anion as the ligand.
- the ligand may be one or more selected from the group consisting of a terephthalic acid anion, a furan dicarboxylic acid anion, a pyridine dicarboxylic acid anion, a benzenetricarboxylic acid, a thiophene dicarboxylic acid anion, and a pyrazole dicarboxylic acid anion.
- the secondary battery according to the present invention may further include a second organic-inorganic hybrid nanoporous material, of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less (herein, p0 represents a saturated vapor pressure at an application temperature and p represents a vapor pressure upon adsorption).
- a second organic-inorganic hybrid nanoporous material of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less (herein, p0 represents a saturated vapor pressure at an application temperature and p represents a vapor pressure upon adsorption).
- second organic-inorganic hybrid nanoporous material may refer to, as described above, an organic-inorganic hybrid nanoporous material of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less.
- the second organic-inorganic hybrid nanoporous material may be an organic-inorganic hybrid nanoporous material having a coordinatively unsaturated metal site present in the framework, surface, or nanopore.
- the usable second organic-inorganic hybrid nanoporous material is not limited to the kind thereof, as long as it has a coordinatively unsaturated metal site (CUS).
- the coordinatively unsaturated metal site may be formed in the framework, or formed on the surface of the second organic-inorganic hybrid nanoporous material or in a metal ion or an organic metal compound present in the nanopore.
- the coordinatively unsaturated metal site refers to a position as a site for the coordination of metals where a ligand coordinated by the metal ions of the organic-inorganic hybrid nanoporous material, representatively water, an organic solvent, etc., are removed, in which another ligand may form a coordination again.
- the coordinatively unsaturated metal site may be formed by partial or entire removal of water, solvent molecules other than water, or ligands, which are contained in the organic-inorganic hybrid nanoporous material.
- a pretreatment of removing water or solvent components bound to the coordinatively unsaturated metal site may be preferably performed.
- any method that may remove water or solvent components may be used as long as it does not induce a modification of the organic-inorganic hybrid nanoporous material.
- the pretreatment may be achieved by heating at a temperature of 100° C. or higher, preferably 150° C.
- the second organic-inorganic hybrid nanoporous material of which the coordinatively unsaturated metal site may be secured by the heat treatment, may include MIL-100, MIL-101, MOF-74, Cu-BTC, MIL-127, CPO-27, etc.
- the second organic-inorganic hybrid nanoporous material may have the coordinatively unsaturated metal site with a density of 0.2 mmol/g to 10 mmol/g. If the density of the coordinatively unsaturated metal site of the second organic-inorganic hybrid nanoporous material is less than 0.2 mmol/g, its nitrogen adsorption capacity is low although having adsorption selectivity for nitrogen, and thus efficiency of a process of separating nitrogen-containing gas is reduced.
- the density of the coordinatively unsaturated metal site of the second organic-inorganic hybrid nanoporous material is more than 10 mmol/g, there is a structural difficulty in the formation of the organic-inorganic hybrid nanoporous material and the density is difficult to achieve experimentally.
- the second organic-inorganic hybrid nanoporous material may include one or more metal ions selected from the group consisting of chromium ion, iron ion, nickel ion, cobalt ion, molybdenum ion, manganese ion, copper ion, magnesium ion, zinc ion, and zirconium ion as the central metal ion.
- the second organic-inorganic hybrid nanoporous material may be prepared by using an organic ligand constituting the general organic-inorganic hybrid nanoporous material without limitation.
- an organic ligand constituting the general organic-inorganic hybrid nanoporous material without limitation.
- 1,4-benzenedicarboxylic acid BDCA
- isophthalic acid 1,3,5-benzenetricarboxylic acid
- BTCA 2,5-dihydroxyterephthalic acid (or 2,5-dihydroxy-1,4-benzene dicarboxylic acid)
- 2-aminoterephthalic acid 2-nitroterephthalic acid, 2-methylterephthalic acid, 2-haloterephthalic acid
- azobenzene tetracarboxylic acid 1,3,5-tri(4-carboxyphenyl)benzene, 2,6-naphthalene dicarboxylic acid (NDCA), benzene-1,3,5-tribenzoic acid (BTB), fumaric acid, glutaric acid,
- 1,4-benzenedicarboxylic acid 1,3,5-benzenetricarboxylic acid, 2,5-dihydroxyterephthalic acid, 2,6-naphthalenedicarboxylic acid, azobenzene tetracarboxylic acid, or derivatives thereof may be used, but is not limited thereto.
- LiPF 6 lithium salts when LiPF 6 lithium salts are included in the electrolyte, LiPF 6 should exist in the form of Li + and PF 6 ⁇ ions. However, without intention, a side reaction occurs, and as a result, PF 5 is produced as a by-product, and reacts with H 2 O which is present in a small amount in the electrolyte to generate HF. HF destroys SEI layer and causes dissolution of a cathode. This phenomenon occurs more remarkably at a high temperature. According to the kind of the lithium salt used as the electrolyte, materials such as HF, HCl, HBr, HI, etc. are produced, in addition to HF, and they act as an acid like HF to generate the problem. Therefore, it is necessary to prevent generation of acids such as HF, etc. by adding the water adsorbent.
- the first organic-inorganic hybrid nanoporous material or second organic-inorganic hybrid nanoporous material according to the present invention may adsorb not only water but also carbon dioxide and/or HF.
- amino groups when amino groups are present in the first organic-inorganic hybrid nanoporous material or second organic-inorganic hybrid nanoporous material, they may also adsorb HF or CO 2 .
- water present inside the battery is electrochemically decomposed, causing a problem of a resistance increase in the battery, and also has a great influence on decomposition of electrolyte.
- preparation of electrode materials and electrolytes are carried out under a water-controlled environment. Since the electrolyte is prepared in a closed system, it is possible to control the content of water at a predetermined level.
- the electrode materials show different water adsorption properties due to an increase of specific surface area and a difference in water affinity depending on the material.
- the secondary battery having the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention as the water adsorbent may have a battery case which accommodates an electrode assembly including a cathode, an anode, and a separator disposed between the cathode and the anode, together with an electrolyte, but is not limited thereto.
- the organic-inorganic hybrid nanoporous material according to the present invention may be included in one or more selected from the group consisting of the cathode, the anode, the separator, the electrolyte, and the interior of the battery case, but is not limited thereto.
- a method of manufacturing the secondary battery according to the present invention may include the step of adsorbing water during manufacturing of the battery and desorbing water during assembling of the battery by using the first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70%, or more, preferably 80% or more of the total adsorption amount of adsorbed water at 150° C. or lower.
- the method of manufacturing the secondary battery according to the present invention may further include the step of disposing the second organic-inorganic hybrid nanoporous material, of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less, in the position where water generated during operation of the battery is adsorbed.
- the first organic-inorganic hybrid nanoporous material may be disposed in the position where water is adsorbed and desorbed during manufacturing of the battery, and the second organic-inorganic hybrid nanoporous material may be disposed in the position where water generated during operation of the battery is adsorbed.
- the second organic-inorganic hybrid nanoporous material may be positioned inside the electrode active material, on the surface of the separator, or inside the electrolyte, together with the first organic-inorganic hybrid nanoporous material.
- the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention as the water adsorbents are applied to the secondary battery
- the first organic-inorganic hybrid nanoporous material and the second organic-inorganic hybrid nanoporous material according to the present invention may be added to the electrolyte or electrode active material composition in an amount of 1 ⁇ 10% by weight, preferably in an amount capable of adsorbing water of 1000 ppm or less, and more preferably, in an amount capable of adsorbing water of 500 ppm or less, respectively.
- the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material may be disposed in the cathode, the anode, the separator, and/or the internal surface of the battery case, or may be included by supporting or coating the materials on a polymer sheet.
- the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention may be coated or deposited on the surface.
- a thickness of the coating layer may be 0.1 micrometer or more to 8.0 micrometer or less. Out of the above range, if the thickness of the coating layer is less than 0.1 micrometer, the desired swelling-preventing effect may not be achieved, and if the thickness of the coating layer is more than 0.8 micrometer, a flow of ions may be disturbed, which is undesirable.
- the secondary battery according to the present invention may be a pouch-type battery having an electrode assembly which is mounted in a pouch-type case made of a laminate sheet including a metal layer and a resin layer.
- the battery case may be constituted by a laminate sheet consisting of an outer cover layer as a polymer film, a barrier layer as a metal film, and a polyolefin-based inner sealant layer.
- the polymer sheet to which the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention are supported may be simply inserted into the corresponding region between the batter case and the electrode assembly during assembling of the battery, or may be attached to the corresponding region of the battery case. In the latter case, the polymer sheet may be attached by using a non-reactive adhesive which does not influence operation of the battery or by thermal fusion.
- the non-reactive adhesive may be a silicone polymer adhesive or a carbon optical fiber polymer adhesive.
- the polymer sheet may be in the form of a non-woven fabric, and a material of the polymer sheet may be PE (polyethylene), PP (polypropylene), PS (polystyrene), PVdF (polyvinylidene fluoride), PTFE (polytetrafluoroethylene), PET (polyethylene-terephthalate). PMMA (polymethylmethacrylate), and/or PAN (polyacrylonitrile).
- PE polyethylene
- PP polypropylene
- PS polystyrene
- PVdF polyvinylidene fluoride
- PTFE polytetrafluoroethylene
- PET polyethylene-terephthalate
- PMMA polymethylmethacrylate
- PAN polyacrylonitrile
- a method of applying the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention to the polymer sheet is not particularly limited, and for example, the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material may be supported in the polymer sheet by a method of immerging the polymer sheet in a solution in which the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material are dispersed, or they may be coated on the surface of the polymer sheet by various methods such as flow coating, spin coating, dip coating, bar coating, etc., or the organic-inorganic hybrid nanoporous materials may be deposited on the surface of the polymer sheet by vaporizing the organic-inorganic hybrid nanoporous materials.
- a particle size and a particle distribution of the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention are not particularly limited, as long as they may exhibit the desired water adsorption function and may not influence performances of the battery.
- the particle size and the particle distribution may be determined by considering their amounts to be loaded on the surface of the electrode assembly or in the battery case, a volume of the battery, etc.
- the particle size of the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention may be, for example, 0.001 ⁇ m to 200 ⁇ m to avoid clogging of separator pores without unnecessarily increasing the volume of the battery.
- the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention are disposed as a coating layer on a part or all of the outer surface of the electrode assembly, they may be dispersed in an organic solvent, together with a binder, to form a slurry, which may be coated on a part or all of the outer surface of the electrode assembly.
- the coating method is not particularly limited, as long as it is a coating method commonly used in the art. For example, a spray coating method may be used.
- the binder polymer may be, for example, one or more selected from the group consisting of polyethylene oxide, polyvinylidene fluoride, polyvinylidene fluoride-hexafluoropropylene, polyvinylidene fluoride-trichlorethylene, polymethyl methacrylate, polyacrylonitrile, polyacrylonitrile-styrene copolymer, polyvinyl chloride (PVC), polyvinyl pyrrolidone, polyvinyl acetate, a polyethylene vinyl acetate copolymer, gelatin, cyanoethylpullulan, cyanoethylpolyvinyl alcohol, cyanoethylcellulose, cyanoethyl sucrose, pullulan, cellulose acetate, cellulose acetate butyrate, cellulose acetate propionate, polyethylene glycol, glyme, polyethylene glycol dimethyl ether, and carboxymethyl cellulose, but is not limited thereto.
- the structure should be composed of a material which is unreactive with the electrolyte to accommodate the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material.
- the structure may be in the form of a bag prepared by using a polyolefin-based non-woven fabric, and after accommodating the organic-inorganic hybrid nanoporous materials, the bag may be sealed by a common method in the art, such as heat seal.
- the prepared structure including the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material may be disposed in a desired position in the battery.
- the position of the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention in the battery is not particularly limited, as long as they are able to adsorb water in the electrolyte in that position.
- the structure supporting the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material may be disposed in upper and lower ends of a jelly-roll type electrode assembly in which the cathode, the separator, and the anode are wound, or in the cross-section of a folded battery in which the cathode, the separator, and the anode are folded, or the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material may be applied to the outer surface of the jelly-roll type electrode assembly, to the outer surface of the folded battery, or inside the battery case by a coating method.
- the first organic-inorganic hybrid nanoporous material, and optionally, the second organic-inorganic hybrid nanoporous material according to the present invention may constitute the laminate material itself constituting the battery case or the electrode assembly.
- an electrode assembly of a cathode/separator/anode structure is mounted in a battery case.
- the lithium secondary battery consists of the cathode, anode, separator, and lithium salt-containing non-aqueous electrolyte, etc.
- the cathode is prepared, for example, by applying and drying a mixture of a cathode active material, a conductive material, and a binder on a cathode current collector. As desired, the mixture may further include a filler.
- the anode is also prepared by applying and drying a anode material on a anode current collector. As desired, the above-described components may be further included.
- the cathode active material may include layered compounds such as lithium cobalt oxide (LiCoO 2 ) and lithium nickel oxide (LiNiO 2 ), or compounds substituted with one or more transition metals; lithium manganese oxides such as compounds of Formula Li 1+x Mn 2 O 4 (wherein x is 0 ⁇ 0.33), LiMnO 3 , LiMn 2 O 3 .
- LiMnO 2 etc.
- lithium copper oxide Li 2 CuO 2
- vanadium oxides such as LiV 3 O 8 , LiFe 3 O 4 , V 2 O 5 , Cu 2 V 2 O 7 , etc.
- the anode active material may include, for example, carbon and graphite materials, such as natural graphite, artificial graphite, expanded graphite, carbon fiber, hard graphitizable carbon, carbon black, carbon nanotube, fullerene, activated carbon, etc.; metals, such as Al, Si, Sn, Ag, Bi, Mg, Zn, In, Ge, Pb, Pd, Pt, Ti which may be alloyed with lithium, and a compound containing these elements; a complex of a metal and a compound thereof and carbon and graphite materials; lithium-containing nitrides, etc.
- a carbon-based active material, a silicon-based active material, a tin-based active material, or a silicon-carbon-based active material is more preferred. These materials may be used alone or in combination of two or more thereof.
- the separator generally has a pore diameter of 0.01 ⁇ m to 10 ⁇ m and a thickness of 5 ⁇ m to 300 ⁇ m.
- sheets or non-woven fabrics made of an olefin polymer such as polypropylene, glass fibers, or polyethylene, which have chemical resistance and hydrophobicity, are used.
- the electrolyte may also serve as the separator.
- binder examples include polyvinyl alcohol, carboxymethylcellulose (CMC), starch, hydroxypropylcellulose, regenerated cellulose, tetrafluoroethylene, polyethylene, polypropylene, ethylene-propylene-diene terpolymer (EPDM), sulfonated EPDM, styrene-butadiene rubber, fluorine rubber, various copolymers, high molecular weight polyvinyl alcohol with high degree of hydrolysis, in addition to those described above.
- CMC carboxymethylcellulose
- EPDM ethylene-propylene-diene terpolymer
- EPDM ethylene-propylene-diene terpolymer
- EPDM ethylene-propylene-diene terpolymer
- EPDM ethylene-propylene-diene terpolymer
- sulfonated EPDM styrene-butadiene rubber
- fluorine rubber various copolymers
- the conductive material is a component to further improve conductivity of the electrode active material, and may be added in an amount of 1% by weight to 30% by weight based on a total weight of the electrode mixture.
- the conductive material is not particularly limited as long as it has conductive properties without causing chemical changes in the battery.
- the conductive material may include, for example, graphite such as natural graphite or artificial graphite; carbon black such as carbon black, acetylene black, ketchen black, channel black, furnace black, lamp black, summer black, etc, carbon derivatives such as carbon nanotubes, fullerene, etc., conductive fibers such as carbon fiber, metal fiber, etc.; metal powder such as carbon fluoride, aluminum, nickel powder, etc; conductive whiskers such as zinc oxide, potassium titanate, etc.; conductive metal oxides such as titanium oxide, etc.; conductive substances such as polyphenylene derivatives, etc.
- graphite such as natural graphite or artificial graphite
- carbon black such as carbon black, acetylene black, ketchen black, channel black, furnace black, lamp black, summer black, etc
- carbon derivatives such as carbon nanotubes, fullerene, etc.
- conductive fibers such as carbon fiber, metal fiber, etc.
- metal powder such as carbon fluoride, aluminum, nickel powder, etc
- a viscosity modifier is a component to adjust the viscosity of the electrode mixture so as to facilitate a mixing process of the electrode mixture and a coating process on a current collector, and may be added in an amount of 30% by weight based on the total weight of the electrode mixture.
- the viscosity modifier include carboxymethylcellulose, polyvinylidene fluoride, etc., but are not limited thereto.
- the above-described solvent may also act as the viscosity modifier.
- a filler is an auxiliary component to inhibit electrode expansion.
- the filler is not particularly limited as long as it is a fibrous material that does not cause chemical changes in the battery, and for example, olefin-based polymers such as polyethylene, polypropylene, etc.; and fibrous materials such as glass fiber, carbon fiber, etc. may be used.
- a coupling agent is an auxiliary component to increase adhesive strength between the electrode active material and the binder, and is characterized by having two or more functional groups.
- the coupling agent may be added in an amount of up to 30% by weight, based on the weight of the binder.
- the coupling agent may be, for example, a material in which one functional group forms a chemical bond via reaction with a hydroxyl or carboxyl group present on the surface of the silicon-, tin- or graphite-based active material, and the other functional group forms a chemical bond via reaction with the polymer binder.
- the coupling agent may include silane-based coupling agents such as triethoxysilylpropyl tetrasulfide, mercaptopropyl triethoxysilane, aminopropyl triethoxysilane, chloropropyl triethoxysilane, vinyl triethoxysilane, methacryloxypropyl triethoxysilane, glycidoxypropyl triethoxysilane, isocyanatopropyl triethoxysilane, cyanatopropyl triethoxysilane, etc., but are not limited thereto.
- silane-based coupling agents such as triethoxysilylpropyl tetrasulfide, mercaptopropyl triethoxysilane, aminopropyl triethoxysilane, chloropropyl triethoxysilane, vinyl triethoxysilane, methacryloxypropyl triethoxysilane, glycidoxy
- An adhesive accelerator is an auxiliary component to improve adhesive strength of the active material to the current collector, and may be added in an amount of 10% by weight or less, based on the weight of the binder.
- Examples of the adhesive accelerator may include oxalic acid, adipic acid, formic acid, acrylic acid derivatives, itaconic acid derivatives, etc.
- a molecular weight regulator may be t-dodecylmercaptan, n-dodecylmercaptan, n-octylmercaptan, etc.
- a crosslinking agent may be 1,3-butanediol diacrylate, 1,3-butanediol dimethacrylate, 1,4-butanediol diacrylate, 1,4-butanediol dimethacrylate, aryl acrylate, aryl methacrylate, trimethylol propane triacrylate, tetraethylene glycol diacrylate, tetraethylene glycol dimethacrylate, divinyl benzene, etc.
- the current collector is a site where migration of electrons takes place in the electrochemical reaction of the active material, and includes a anode current collector and a cathode current collector according to the kind of the electrode.
- the anode current collector is generally fabricated in a thickness of 3 ⁇ m to 500 ⁇ m.
- the anode current collector is not particularly limited, as long as it has conductivity without causing chemical changes in the battery.
- copper, stainless steel, aluminum, nickel, titanium, sintered carbon, copper or stainless steel having a surface treated with carbon, nickel, titanium or silver, aluminum-cadmium alloys, etc. may be used.
- the cathode current collector is generally fabricated in a thickness of 3 ⁇ m to 500 ⁇ m.
- the cathode current collector is not particularly limited, as long as it has high conductivity without causing chemical changes in the battery.
- stainless steel, aluminum, nickel, titanium, sintered carbon, aluminum or stainless steel having a surface treated with carbon, nickel, titanium or silver, etc. may be used.
- These current collectors may also be processed to form fine irregularities on the surfaces thereof so as to enhance adhesive strength to the electrode active materials.
- the current collectors may be used in various forms including films, sheets, foils, nets, porous structures, foams, non-woven fabrics, etc.
- the lithium-containing non-aqueous electrolyte is composed of a non-aqueous electrolyte and lithium salt.
- non-protic organic solvents such as N-methyl-2-pyrollidinone, propylene carbonate, ethylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, gamma-butyro lactone, 1,2-dimethoxy ethane, tetrahydroxy Franc, 2-methyl tetrahydrofuran, dimethylsulfoxide, 1,3-dioxolane, formamide, dimethylformamide, dioxolane, acetonitrile, nitromethane, methyl formate, methyl acetate, phosphoric acid triester, trimethoxy methane, dioxolane derivatives, sulfolane, methyl sulfolane, 1,3-dimethyl-2-imidazolidinone, propylene carbonate derivatives, tetrahydrofuran derivatives, ether, methyl propionate, ethyl propionate, etc.
- non-protic organic solvents such as N-methyl-2
- the lithium salt is a material that is readily soluble in the non-aqueous electrolyte, and for example, LiCl, LiBr, LiI, LiClO 4 , LiBF 4 , LiB 10 Cl 10 , LiPF 6 , LiCF 3 SO 3 , LiCF 3 CO 2 , LiAsF 6 , LiSbF 6 , LiAlC 4 , CH 3 SO 3 Li, CF 3 SO 3 Li, (CF 3 SO 2 ) 2 NLi, chloroborane lithium, lower aliphatic carboxylic acid lithium, lithium tetraphenyl borate, imide, etc. may be used.
- an organic solid electrolyte an inorganic solid electrolyte, etc. may be used.
- the organic solid electrolyte may include, for example, polyethylene derivatives, polyethylene oxide derivatives, polypropylene oxide derivatives, phosphoric acid ester polymer, poly agitation lysine, polyester sulfide, polyvinyl alcohol, poly(vinylidene fluoride), and polymers containing ionic dissociation groups, etc.
- the inorganic solid electrolyte may include, for example, nitrides, halides, and sulfates of Li, such as Li 3 N, LiI, Li 5 NI 2 , Li 3 N—LiI—LiOH, LiSiO 4 , LiSiO 4 —LiI—LiOH, Li 2 SiS 3 , Li 4 SiO 4 , Li 4 SiO 4 —LiI—LiOH, Li 3 PO 4 —Li 2 S—SiS 2 , etc.
- Li such as Li 3 N, LiI, Li 5 NI 2 , Li 3 N—LiI—LiOH, LiSiO 4 , LiSiO 4 —LiI—LiOH, Li 2 SiS 3 , Li 4 SiO 4 , Li 4 SiO 4 —LiI—LiOH, Li 3 PO 4 —Li 2 S—SiS 2 , etc.
- pyridine triethylphosphite, triethanolamine, cyclic ether, ethylenediamine, n-glyme, hexaphosphoric triamide, nitrobenzene derivatives, sulfur, quinone imine dyes, N-substituted oxazolidinone, N,N-substituted imidazolidine, ethylene glycol dialkyl ether, ammonium salts, pyrrole, 2-methoxy ethanol, aluminum trichloride or the like may be added to the non-aqueous electrolyte.
- the non-aqueous electrolyte may further include halogen-containing solvents such as carbon tetrachloride, ethylene trifluoride, etc. in order to impart incombustibility, and may further include carbon dioxide gas in order to improve high-temperature storage characteristics.
- halogen-containing solvents such as carbon tetrachloride, ethylene trifluoride, etc.
- carbon dioxide gas in order to improve high-temperature storage characteristics.
- the lithium secondary battery according to the present invention may be manufactured by a common method known in the art.
- the structures of the cathode, the anode, and the separator are not particularly limited, and for example, the lithium secondary battery has a structure in which respective sheets may be inserted into a cylindrical, rectangular, or pouch case in a winding type or a folding or stacking type.
- the lithium secondary battery according to the present invention may be preferably used as a high-power large-scale battery or a unit battery for a battery pack.
- the battery pack may be particularly used as a power source for vehicles such as electric vehicles requiring excellent high-temperature storage characteristics, hybrid electric vehicles, power tool plug-in hybrid electric vehicles, power storage devices, etc.
- Al(OH)BDC aluminum 2,5-furanedicarboxylate
- FIG. 2 shows X-ray diffraction pattern and X-ray pattern measured by using synthesized Al(OH)BDC powder.
- Al(OH)BDC has Chemical Formula of [Al(OH)[(O 2 C)—C 6 H 4 —(CO 2 )].n (solvent) (wherein the solvent is H 2 O, and n is a real number ranging from 0.1 to 10), and Al(OH)BDC after being dried at 150° C. or higher has Chemical Formula of [Al(OH)[(O 2 C)—C 6 H 4 —(CO 2 )], and it was calculated that dried Al(OH)BDC has a molecular weight of about 204 g/mol.
- the framework structure of Al(OH)BDC may be built from inorganic aluminum chains linked via carboxylate groups from the ligands, and the chains may be described as AlO 6 octahedra cis-connected by corner. Each octahedra is surrounded by four oxygen atoms derived from four carboxylate ligands and oxygen atoms derived from two OH groups. The two OH ⁇ ion groups linked to Al of AlO 6 octahedra are in cis-position and bridge the Al centers to create the chains. As shown in FIG. 1 , the nanopore structure of Al(OH)BDC forms square-shaped sinusoidal channels having a diameter of about 7 ⁇ .
- a TriStar volume adsorption device manufactured by Micrometrics was used to perform a nitrogen physical adsorption experiment at ⁇ 196° C., and shown in FIG. 4 .
- the Al(OH)BDC material was dried at a vacuum level of 10 ⁇ 4 Torr or higher and a pretreatment temperature of 150° C. for 6 hours, and then a nitrogen adsorption amount was measured.
- a physical adsorption isotherm of nitrogen thus obtained showed Type-I isotherm as in nanoporous zeolite, and a calculated BET surface area and a nanopore volume were 650 m 2 /g and 0.27 cm 3 /g, respectively.
- a water adsorption property of the Al(OH)BDC material was measured by using an IGA gravimetric adsorption analyzer manufactured by Hiden.
- the Al(OH)BDC material was dried at a vacuum level of 10 ⁇ 5 Torr and a temperature of 150° C. for 6 hours, and then temperature was decreased to 30° C. to measure adsorption and desorption isotherms at a ratio of water vapor pressure to saturated vapor pressure (p/p0) ranging from 0 ⁇ 1.0.
- the water adsorption/desorption isotherms of Al(OH)BDC as shown in FIG. 5 has a characteristic of having S-shaped reversible isotherm in an almost saturated form at p/p0>0.20.
- Al(OH)BDC showed a high adsorption amount close to 0.30 g per 1 g.
- a thermogravimetric analysis of FIG. 3 confirmed that 24% by weight of the Al(OH)BDC material saturated with water was dehydrated at a low temperature of 90° C. or lower.
- Al—OH groups in the framework of Al(OH)BDC increase hydrophilicity of the organic-inorganic hybrid nanoporous material and also interact with water molecules in an appropriate strength, and therefore, the Al(OH)BDC material is regenerable at a much lower temperature, compared to zeolite.
- An organic-inorganic hybrid Al-Fumarate was synthesized as follows. 70 ml of water (H 2 O) was put in a beaker, and 15.06 g of aluminum sulfate salt hydrate (Al 2 (SO 4 ) 3 .18H 2 O) was added thereto to prepare a first solution. 70 ml of water (1H 2 O) was put in a beaker, and 5.2 g of fumaric acid and 5.3 g of sodium hydroxide (NaOH) were added thereto to prepare a second solution. After the solutions were completely dissolved, the second solution was slowly added to the first solution and stirred for 30 minutes while maintaining the two solutions at 60° C.
- Al-Fumarate after the synthesis has Chemical Formula of [Al(OH)[(O 2 C)—C 2 H 2 —(CO 2 )].n (solvent) (wherein the solvent is H 2 O), and Al-Fumarate after being dried at 100° C. has Chemical Formula of [Al(OH)[(O 2 C)—C 2 H 2 —(CO 2 )].
- solvent wherein the solvent is H 2 O
- Al-Fumarate after being dried at 100° C. has Chemical Formula of [Al(OH)[(O 2 C)—C 2 H 2 —(CO 2 )].
- thermogravimetric analysis of the Al-Fumarate material obtained by the synthesis confirmed that the adsorption amount calculated from the water amount desorbed at 100° C. or lower was up to 0.53 g/g, indicating applicability of the material as a water adsorbent. Further, the rapid weight reduction at 400-450° C. was caused by a weight reduction due to destruction of the crystal structure, and Al-Fumarate was confirmed to be thermally stable up to 400° C.
- the Al-Fumarate material was treated at a pretreatment temperature of 150° C. for 12 hours, and then a physical adsorption of nitrogen was measured at ⁇ 196° C.
- An organic-inorganic hybrid nanoporous material, Al-FDC was synthesized as follows. First, 30 mmol of 2,5-furan dicarboxylic acid, 30 mmol of AlCl 3 .6H 2 O, 30 mmol of NaOH, and 60 mL of deionized water were placed in a 100 ml-3 neck round bottom flask, and mixed with each other at room temperature for 3 hours, followed by heating at 100° C. under stirring at reflux for 24 hours. After being cooled to room temperature, a product was recovered by centrifugation.
- the organic-inorganic hybrid nanoporous materials are known to have different structures and material compositions depending on coordination and bond formation, even though they are composed of the same metal ions and organic ligands.
- X-ray diffraction patterns measured by using Al-FDC powder were the same as the patterns suggested in Advanced materials, Vol 27(32), 4775-4780, 2015.
- the Al-FDC material has Chemical Formula of [Al(OH)[(O 2 C)—C 4 OH 2 —(CO 2 )].n (solvent) (wherein the solvent is H 2 O, and n is a real number ranging from 0.1 to 10), and Al-FDC after being dried at 150° C. or higher has Chemical Formula of [Al(OH)[(O 2 C)—C 4 OH 2 —(CO 2 )].
- a BET surface area was 1070 m 2 /g, and a nanopore volume was 0.398 cm 3 /g.
- a water adsorption property of the Al-FDC material was measured by using an IGA gravimetric adsorption analyzer manufactured by Hiden.
- the Al-FDC material was dried at a vacuum level of 10 ⁇ 5 Torr and a temperature of 150° C. for 6 hours, and then temperature was decreased to 30° C. to measure adsorption and desorption isotherms at a ratio of water vapor pressure to saturated vapor pressure (p/p0) ranging from 0 ⁇ 1.0.
- the water adsorption/desorption isotherms of Al-FDC has a characteristic of having S-shaped reversible isotherm in an almost saturated form at p/p0 ⁇ 0.20, as in the above-mentioned Advanced materials, Vol 27(32), 4775-4780, 2015. In this range, Al-FDC showed a high adsorption amount close to 0.35 g per 1 g.
- the Al—OH groups and polar heterocyclic organic ligands in the framework of Al-FDC increase hydrophilicity of the organic-inorganic hybrid nanoporous material and also interact with water molecules in an appropriate strength, and therefore, the Al-FDC material is regenerable at a much lower temperature, compared to zeolite.
- An organic-inorganic hybrid nanoporous material, Iron benzenetricarboxylate (MIL-100(Fe)) was synthesized as follows. First, Fe(NO 3 ) 3 .9H 2 O (10.33 g), 1,3,5-benzenetricarboxylic acid (3.6 g), and 10.2 mL of H 2 O were reacted in a 100 mL microwave reactor (MARS-5) at 180° C. for 1 hour. To remove unreacted ligand residues, the synthesized compound was washed with an excessive amount of ethanol, and filtered and dried.
- MIL-100(Fe) Iron benzenetricarboxylate
- MIL-100(Fe) material obtained by the synthesis has Chemical Formula of [Fe 2 O(OH)[(O 2 C)—C 6 H 4 —(CO 2 )].n (solvent) (wherein the solvent is H 2 O), and MIL-100(Fe) after being dried at 100° C. has Chemical Formula of [Fe 3 O(OH)[(O 2 C)—C 6 H 4 —(CO 2 )]. With regard to a structure of MIL-100(Fe) calculated by X-ray diffraction analysis, as shown in FIG.
- thermogravimetric analysis of MIL-100(Fe) material obtained by the synthesis is shown in FIG. 10 .
- 40.7% of water was desorbed at 100° C. or lower, and weight loss occurred in the range of 100° C. to 400° C., which is attributed to water strongly adsorbed or water desorbed from metal clusters, suggesting that the MIL-100(Fe) organic-inorganic hybrid nanoporous material has a site strongly adsorbing water.
- the MIL-100(Fe) material was treated at a pretreatment temperature of 250° C. for 6 hours, and then a nitrogen physical adsorption experiment was performed at ⁇ 196° C., and water adsorption/desorption isotherms were measured at 30° C.
- the water adsorption amount was up to 0.74 g/g, indicating applicability as a water adsorbent.
- LiFePO 4 cathode active material Alfa
- Al-Fumarate, and MIL-100(Fe) organic-inorganic hybrid nanoporous materials which were prepared in Examples 1, 2, and 3, respectively at a weight ratio of 10% to prepare cathode active materials mixed with the organic-inorganic hybrid nanoporous materials.
- thermogravimetric analyzer connected with a relative humidity-controllable air injector was used to perform a test.
- the test sample was loaded on the analyzer, and then air containing water at a relative humidity of 10% was injected into the test sample until equilibrium was reached, and the sample was saturated with water so that the weight change was 0.02% or less.
- temperature of the plate on which the test sample was loaded was raised to 60° C., 80° C., 120° C., a water desorption amount was examined. Thereafter, when temperature was decreased to 30° C., a water adsorption amount was examined.
- the organic-inorganic hybrid nanoporous material is an adsorbent for a secondary battery capable of effectively removing a trace amount of water during assembling or operating of the secondary battery. As shown in FIG.
- the water adsorption amount of the Al-Fumarate adsorbent under dry condition was 50% of that of Al(OH)BDC, indicating applicability of the Al-Fumarate adsorbent as a water adsorbent for secondary batteries. As shown in FIG.
- adsorption capacity of MIL-100 at a relative humidity of 10% was 0.050 g/g MOF, and a desorption rate under dry condition was 32% (0.016 g/g MOF).
- MIL-100 adsorbent also showed strong water adsorption strength at a relative humidity of 10, or less, similar to Al-Fumarate adsorbent.
- the water adsorption amount of MIL-100 adsorbent under dry condition was 0.034 g/g MOF, which was higher than that of Al(OH)BDC.
- An anode mixture slurry was prepared by mixing 94 wt % of carbon powder having an average diameter of 20 ⁇ m as an anode active material, 2 wt % of Al-FDCA powder having an average diameter of 0.5 ⁇ m to 1 ⁇ m, 1 wt % of carbon black as a conductive material, and 3 wt % of polyvinylidene fluoride (PVdF) as a binder, followed by adding the mixture to a solvent N-methyl-2-pyrrolidone (NMP).
- NMP solvent N-methyl-2-pyrrolidone
- a cathode mixture slurry was prepared by mixing 92 wt % of lithium cobalt oxide (LiCoO2) powder having an average diameter of 2 ⁇ m to 5 ⁇ m as a cathode active material, 2 wt % of Al-FDCA powder having an average diameter of 0.5 ⁇ m to 1 ⁇ m, 3 wt % of carbon black as a conductive material, and 3 wt % of polyvinylidene fluoride (PVdF) as a binder, followed by adding the mixture to a solvent N-methyl-2-pyrrolidone (NMP).
- NMP solvent N-methyl-2-pyrrolidone
- PVdF-CTFE polymer polyvinylidene fluoride-co-chlorotrifluoroethylene polymer
- a polymer solution about 5 wt % of polyvinylidene fluoride-co-chlorotrifluoroethylene polymer (PVdF-CTFE polymer) was added to acetone and dissolved at 50° C. for at least 12 hours to prepare a polymer solution.
- Solid Al-FDCA at a concentration of about 10 wt % was added to the thus-prepared polymer solution, and pulverized and dispersed for at least 12 hours using a ball mill method to prepare a slurry.
- the Al-FDCA powder having an average diameter of 0.5 ⁇ m to 1 ⁇ m, was added to prepare the slurry.
- the slurry was then coated on the surface of the roll to a thickness of about 15 ⁇ m using a spray coating method and was dried.
- An anode mixture slurry was prepared by mixing 96 wt % of carbon powder having an average diameter of 20 pin as an anode active material, 1 wt % of carbon black as a conductive material, and 3 wt % of polyvinylidene fluoride (PVdF) as a binder, followed by adding the mixture to a solvent N-methyl-2-pyrrolidone (NMP).
- PVdF polyvinylidene fluoride
- NMP solvent N-methyl-2-pyrrolidone
- a cathode mixture slurry was prepared by mixing 94 wt % of lithium cobalt oxide (LiCoO2) powder having an average diameter of 2 ⁇ m to 5 ⁇ m as a cathode active material, 3 wt % of carbon black as a conductive material, and 3 wt % of polyvinylidene fluoride (PVdF) as a binder, followed by adding the mixture to a solvent N-methyl-2-pyrrolidone (NMP).
- NMP solvent N-methyl-2-pyrrolidone
- VdF-CTFE polymer polyvinylidene fluoride-co-chlorotrifluoroethylene polymer
- LiPF6 lithium hexafluorophosphate
- the prepared secondary battery was charged at a fixed current of 1 C until it reached 4.2 V, and further charged for 4 hours under a fixed charging condition of 4.2 V.
- the battery was then discharged at a current of 1200 mA until the voltage thereof reached 3.0 V.
- the stability index was 54%
- the secondary battery including organic-inorganic hybrid nanoporous materials as the adsorbent showed a stability index of 93%, indicating a stable charge/discharge capacity.
- a first organic-inorganic hybrid nanoporous material which may be regenerated by desorbing 70% or more, preferably 80% or more of a total adsorption amount of adsorbed water at 150° C. or lower according to the present invention is used as a water adsorbent for a secondary battery
- high water adsorption capacity may be achieved, and water adsorbed by the water adsorbent during manufacturing of the secondary battery may be desorbed by vacuum treatment at 150° C. or lower during assembling of the battery, thereby being removed from the battery.
- a second organic-inorganic hybrid nanoporous material of which water adsorption capacity is higher than water desorption capacity at a relative humidity p/p0 of 0.3 or less, is further used in addition to the first organic-inorganic hybrid nanoporous material, gas components which may be generated during operation of the battery may be effectively adsorbed and may not be desorbed. Accordingly, side-reactions by water may be prevented, thereby improving reliability of the battery. Further, deterioration of storage and life-time characteristics of the battery due to swelling by carbon dioxide may be prevented.
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